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020 _aTHE0007799(Local)
039 9 _a201906131120
_bnadia
_c201705171042
_dfateeha
_y201705031211
_zfateeha
040 _aUMP
090 _aFIST .A36 2017 r Thesis
100 0 _aNor Ain Syuhada Zuhaimi
245 1 0 _aGypsum based catalysts for the catalytic synthesis of glycerol carbonate /
_cNor Ain Syuhada Zuhaimi
260 _aKuantan, Pahang :
_bUMP,
_c2017
300 _axv, 121 p. :
_bill. (some col.) ;
_c30 cm. +
_e1 CD-ROM
500 _aFaculty of Industrial Sciences and Technology
502 _aThesis (Master of Science (Industrial Chemistry)) -- Universiti Malaysia Pahang – 2017
504 _aBibliography : p. 104-117
520 3 _aSynthesis of glycerol carbonate from glycerol has attracted the interest from many researchers across the world due to their interesting chemical properties. However, the tremendous growth of biodiesel have make drop of glycerol’s price due to the excessive production of glycerol. Therefore, researchers find it necessary to tune this chemical into a value added compound such as glycerol carbonate. In this study, the catalytic carbonylation of glycerol with urea in the presence of treated commercial gypsum and red gypsum as catalyst are reported for the first time. Gypsum (CaSO4•2H2O) is one of the waste materials produced from advanced material industrial processing plant. Red gypsum is an unwanted by-product from titanium dioxide manufacturing industry. The effects of physical and chemical pre-treatment procedures on both gypsums were investigated. To obtain the catalyst structure-activity relationship, the treated catalysts were characterised by means of several characterisation techniques (i.e., XRD, TGA, BET surface area, SEM, CO2–TPD, NH3–TPD and Hammett test). Tunable physicochemical properties of gypsum based catalysts were successfully prepared by varying the pre-treatment techniques, which later on contributed to the variation of catalytic activity toward glycerol carbonate formation from glycerol. The highest catalytic activity obtained was for catalyst consisting β-CaSO4 phase where it produced 83.6% yield of glycerol carbonate for commercial gypsum and 87.4% for red gypsum, respectively. The presence of Ca2+ acts as Lewis acid sites while (SO4)2- acts as conjugate basic sites in gypsum based catalysts is responsible for the catalytic activity. Optimisation for the red gypsum catalyst showed that the suitable parameters for catalytic testing were 150 °C, 340 rpm and 0.25 g (1.81 wt%) with 4 h reaction time respectively. Gypsum catalyst is easily recoverable and reusable for subsequent cycles of reaction. Similar physico-chemical properties of fresh and used catalyst were confirmed through XRD and SEM. Besides, the mechanistic pathway of glycerol carbonate was confirmed through the formation of glycerol carbamate as intermediate compound which was further established through time on-stream analysis study using 13C NMR and ATR–FTIR, respectively. The study clearly supports conversion of waste into wealth while promising proper disposal of waste to produce value added product.
610 2 0 _aFaculty of Industrial Sciences and Technology
_xDissertations
650 0 _aUniversities and Colleges
_xDissertations
650 0 _aTheses
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